CN115491677B - Acidic etching solution for titanium-aluminum-titanium composite film and preparation method thereof - Google Patents
Acidic etching solution for titanium-aluminum-titanium composite film and preparation method thereof Download PDFInfo
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- CN115491677B CN115491677B CN202211160441.9A CN202211160441A CN115491677B CN 115491677 B CN115491677 B CN 115491677B CN 202211160441 A CN202211160441 A CN 202211160441A CN 115491677 B CN115491677 B CN 115491677B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
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Abstract
The invention provides an acidic etching solution for a titanium aluminum titanium composite film layer and a preparation method thereof. The thiosulfate in the acidic etching solution can form a complex with the titanium dioxide to be dissolved in the liquid medicine, so that continuous etching of the metal titanium is promoted, and further etching reaction of the titanium dioxide passivation film is prevented.
Description
Technical Field
The invention relates to the technical field of etching solutions, in particular to an acidic etching solution for a titanium-aluminum-titanium composite film layer and a preparation method thereof.
Background
The grid electrode, the source electrode and the drain electrode of the liquid crystal display panel structure are usually made of aluminum materials, but the adhesion of pure aluminum to base materials (usually silicon oxide and silicon nitride) is poor, so that a transition layer is required to be added between an aluminum film and a base to enhance the adhesion between laminated metal and a base material, and a protective layer is required to be added on the surface of the aluminum film to prevent oxidation in the surface of the aluminum film; the transition layer and the protective layer can be titanium film layers, so that a titanium-aluminum-titanium composite film layer is formed.
In order to form a circuit, the titanium aluminum titanium composite film layer needs to be etched, and the common aluminum etching solution mixed by phosphoric acid and nitric acid cannot effectively etch the titanium, because the titanium forms a titanium dioxide passivation film under the action of oxidizing acid to prevent further etching reaction, so fluorine-containing reagents such as hydrofluoric acid, fluoride and the like need to be added. Chinese patent CN110344062a discloses an etching solution for a gate titanium aluminum titanium laminated metal film, the chemical solution comprising nitric acid, an oxidizing acid perchlorate, and fluorides such as ammonium fluoride and hydrogen fluoride. Patent CN102326235a discloses a composite film etching solution with aluminum or aluminum alloy as the upper layer and titanium or titanium alloy as the lower layer, which contains fluoride.
In practical application, the existence of fluoride can effectively corrode titanium or titanium alloy metal, but the existence of fluorine can corrode a base material, so that the composite film layer is collapsed and deformed, and fluorine can corrode equipment of a machine and cause equipment damage.
Disclosure of Invention
In view of the above, the present invention provides an acidic etching solution that can effectively etch a titanium aluminum titanium composite film layer without damaging a substrate material.
The technical scheme of the invention is realized as follows:
in one aspect, the invention provides an acidic etching solution for a titanium aluminum titanium composite film layer, which comprises an oxidizing acid, a non-oxidizing acid, thiosulfate and deionized water.
On the basis of the technical scheme, preferably, the acidic etching solution comprises, by mass percent, 100%, 2% -10% of oxidizing acid, 15% -30% of non-oxidizing acid, 0.2% -2% of thiosulfate and the balance of deionized water.
On the basis of the technical scheme, the method preferably further comprises pyrosulfate.
On the basis of the technical scheme, preferably, the acidic etching solution comprises, by mass, 100%, 2% -10% of oxidizing acid, 15% -30% of non-oxidizing acid, 0.2% -2% of thiosulfate, 0.5% -3% of pyrosulfate and the balance of deionized water.
On the basis of the above technical scheme, preferably, the oxidizing acid is one or a combination of several of nitric acid, hydroiodic acid, perchloric acid, nitrous acid and chromic acid.
On the basis of the technical scheme, preferably, the non-oxidizing acid is one or a combination of more of hydrochloric acid, sulfuric acid and phosphoric acid.
On the basis of the technical scheme, preferably, the thiosulfate is one or two of sodium thiosulfate and potassium thiosulfate.
On the basis of the technical scheme, preferably, the pyrosulfate is one or two of sodium pyrosulfate and potassium pyrosulfate.
On the other hand, the invention provides a preparation method of an acidic etching solution of a titanium aluminum titanium composite film layer, which comprises the steps of adding deionized water into oxidizing acid, stirring uniformly, slowly adding non-oxidizing acid under a stirring state, stirring uniformly again, adding thiosulfate and pyrosulfate, stirring to dissolve, and then filtering the mixed solution by suction, and collecting filtrate to obtain the acidic etching solution.
The acidic etching solution of the titanium aluminum titanium composite film layer has the following beneficial effects compared with the prior art:
(1) The oxidizing acid can oxidize metallic titanium and aluminum into corresponding oxides, and the non-oxidizing acid can effectively dissolve aluminum oxide to promote the continuous reaction; the thiosulfate can form a complex with the titanium dioxide to be dissolved in the liquid medicine, so that the continuous etching of the metal titanium is promoted, and the titanium dioxide passivation film is prevented from stopping further etching reaction.
(2) The pyrosulfate can form soluble titanium sulfate with titanium dioxide and soluble aluminum sulfate with aluminum oxide, so that continuous etching of metallic titanium and aluminum is promoted, and aluminum film shrinkage is avoided.
(3) Thiosulfate and pyrosulfate also have the function of stabilizing the liquid medicine, and prevent the liquid medicine from bumping.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the effect of the acidic etching solution on the corrosion of a substrate when the acidic etching solution is used for effectively etching a titanium aluminum titanium composite film layer;
FIG. 2 is a graph showing the effect of whether delamination occurs when the acidic etching solution of the present invention is used for effectively etching a titanium aluminum titanium composite film layer;
FIG. 3 is a graph showing the stability effect of the acidic etching solution of the present invention.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Example 1
The acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises, by mass, 100% of nitric acid 2%, hydrochloric acid 15%, sodium thiosulfate 0.2%, sodium pyrosulfate 0.5% and deionized water in balance.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises the following steps: adding 53.74g of deionized water into 2.86g of nitric acid with the concentration of 70%, stirring uniformly, slowly adding 41.7g of hydrochloric acid with the concentration of 36% under the stirring state, stirring uniformly again, adding 0.2g of sodium thiosulfate and 0.5g of sodium pyrosulfate, stirring to dissolve, and then carrying out suction filtration on the mixed solution, and collecting filtrate to obtain the acidic etching solution.
Example 2
The acidic etching solution for the titanium aluminum titanium composite film layer in the embodiment comprises, by mass, 100% of nitric acid 2%, perchloric acid 2%, hydrochloric acid 10%, phosphoric acid 12%, sodium thiosulfate 0.5%, potassium thiosulfate 0.5%, sodium pyrosulfate 1% and the balance of water.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises the following steps: 50.36g of deionized water is added into 2.86g of mixed acid of nitric acid with the concentration of 70% and 2.86g of perchloric acid with the concentration of 70%, after stirring uniformly, 27.8g of hydrochloric acid with the concentration of 36% and 14.12g of phosphoric acid with the concentration of 85% are slowly added under stirring, after stirring uniformly again, 0.5g of sodium thiosulfate, 0.5g of potassium thiosulfate and 1g of sodium pyrosulfate are added, stirring is carried out to dissolve the materials, and then the mixed solution is filtered by suction, and the filtrate is collected to obtain the acid etching solution.
Example 3
The acidic etching solution for the titanium aluminum titanium composite film layer in the embodiment comprises, by mass, 100% of 4% of hydriodic acid, 4% of perchloric acid, 10% of hydrochloric acid, 16% of sulfuric acid, 1% of potassium thiosulfate, 0.5% of sodium thiosulfate, 2.5% of sodium pyrosulfate and the balance of water.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises the following steps: 31.12g of deionized water is added into 8.51g of mixed acid of hydroiodic acid with the concentration of 47% and 5.71g of perchloric acid with the concentration of 70%, after stirring uniformly, 27.8g of hydrochloric acid with the concentration of 36% and 22.86g of sulfuric acid with the concentration of 70% are slowly added under stirring, after stirring uniformly again, 1g of potassium thiosulfate, 0.5g of sodium thiosulfate and 2.5g of sodium pyrosulfate are added, stirring is carried out to dissolve the materials, and then the mixed solution is filtered by suction, and the filtrate is collected to obtain the acid etching solution.
Example 4
The acidic etching solution for the titanium aluminum titanium composite film layer in the embodiment comprises, by mass, 100% of nitric acid 2%, chromic acid 4%, hydrochloric acid 10%, phosphoric acid 8%, sodium thiosulfate 0.3%, potassium thiosulfate 0.5%, sodium pyrosulfate 1%, potassium pyrosulfate 0.5% and the balance of water.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises the following steps: 51.28g of deionized water is added into 2.86g of mixed acid of nitric acid with the concentration of 70% and 6.35g of chromic acid with the concentration of 63%, after uniform stirring, 27.8g of hydrochloric acid with the concentration of 36% and 9.41g of phosphoric acid with the concentration of 85% are slowly added under stirring, after uniform stirring again, 0.3g of potassium thiosulfate, 0.5g of sodium thiosulfate, 1g of sodium pyrosulfate and 0.5g of potassium pyrosulfate are added, stirring is carried out to dissolve the materials, and then the mixed solution is filtered by suction, and filtrate is collected to obtain the acidic etching solution.
Example 5
The acidic etching solution for the titanium aluminum titanium composite film layer in the embodiment comprises, by mass, 100% of perchloric acid 4%, chromic acid 6%, hydrochloric acid 10%, sulfuric acid 20%, sodium thiosulfate 1%, potassium thiosulfate 1%, sodium pyrosulfate 1% and potassium pyrosulfate 2%, and the balance of water.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises the following steps: 23.4g of deionized water is added into 5.71g of mixed acid of perchloric acid with the concentration of 70% and 9.52g of chromic acid with the concentration of 63%, after stirring uniformly, 27.8g of hydrochloric acid with the concentration of 36% and 28.57g of sulfuric acid with the concentration of 70% are slowly added under stirring, after stirring uniformly again, 1g of potassium thiosulfate, 1g of sodium pyrosulfate and 2g of potassium pyrosulfate are added, stirring is carried out to dissolve the materials, and then the mixed solution is filtered by suction, and the filtrate is collected to obtain the acid etching solution.
Example 6
This example is identical to example 2, except for the lack of sodium pyrosulfate, and is specifically as follows:
the acidic etching solution for the titanium aluminum titanium composite film layer in the embodiment comprises, by mass, 100% of nitric acid 2%, perchloric acid 2%, hydrochloric acid 10%, phosphoric acid 12%, sodium thiosulfate 0.5%, potassium thiosulfate 0.5% and the balance of water.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises the following steps: 51.36g of deionized water is added into 2.86g of mixed acid of nitric acid with the concentration of 70% and 2.86g of perchloric acid with the concentration of 70%, after uniform stirring, 27.8g of hydrochloric acid with the concentration of 36% and 14.12g of phosphoric acid with the concentration of 85% are slowly added under stirring, after uniform stirring again, 0.5g of sodium thiosulfate and 0.5g of potassium thiosulfate are added, stirring is carried out to dissolve the materials, and then the mixed solution is filtered by suction, and filtrate is collected to obtain the acidic etching solution.
Comparative example 1
Comparative example 1 is identical to example 2, except that thiosulfate is absent, as follows:
the acidic etching solution of the titanium aluminum titanium composite film layer of the comparative example comprises, by mass, 100% of nitric acid 2%, perchloric acid 2%, hydrochloric acid 10%, phosphoric acid 12% and sodium pyrosulfate 1%, with the balance being water.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer of the comparative example comprises the following steps: 51.36g of deionized water is added into 2.86g of mixed acid of nitric acid with the concentration of 70% and 2.86g of perchloric acid with the concentration of 70%, 27.8g of hydrochloric acid with the concentration of 36% and 14.12g of phosphoric acid with the concentration of 85% are slowly added under stirring after uniform stirring, 1g of sodium pyrosulfate is added after uniform stirring again, stirring is carried out to dissolve the mixture, and then the filtrate is collected after suction filtration of the mixture, thus obtaining the acid etching liquid.
Comparative example 2
Comparative example 2 the same as example 2 was different in that thiosulfate and pyrosulfate were composed of ammonium fluoride and hydrogen fluoride in fluoride, wherein 1% of ammonium fluoride and 1% of hydrogen fluoride were as follows:
the acidic etching solution for the titanium aluminum titanium composite film layer in the embodiment comprises, by mass, 100% of nitric acid 2%, perchloric acid 2%, hydrochloric acid 10%, phosphoric acid 12%, ammonium fluoride 1%, hydrogen fluoride 1% and the balance of water.
The preparation method of the acidic etching solution of the titanium aluminum titanium composite film layer in the embodiment comprises the following steps: 48.86g of deionized water is added into 2.86g of mixed acid of nitric acid with the concentration of 70% and 2.86g of perchloric acid with the concentration of 70%, after stirring uniformly, 27.8g of hydrochloric acid with the concentration of 36% and 14.12g of phosphoric acid with the concentration of 85% are slowly added under stirring, after stirring uniformly again, 1g of ammonium fluoride and 2.5g of hydrogen fluoride with the concentration of 40% are added, stirring is carried out to dissolve the materials, and then the mixed solution is filtered by suction, and the filtrate is collected to obtain the acidic etching solution.
Table 1 example and comparative example etchant compositions
Remarks: the oxidizing acid and the non-oxidizing acid in the table are calculated as 100% concentration, and the examples and comparative examples are converted values of common concentrations.
Etching effect test: and (3) plating a titanium film on the glass substrate by a sputtering method for 30nm, further plating an aluminum film by a sputtering method for 600nm, further plating a titanium film by a sputtering method for 70nm to form a titanium aluminum titanium composite film layer, and coating positive photoresist on the surface of the composite film layer and patterning to finish the manufacture of the titanium aluminum titanium composite film layer.
The substrate was etched in the above-mentioned different solutions at 40 ℃, after the etching was completed, the corrosiveness of the solution to the substrate glass (silicon oxide) was observed under SEM, and the cross-sectional shape of the composite film was also observed to confirm whether the composite film had delamination due to uneven etching of titanium and aluminum, and the results are shown in table 2.
Table 2 effects of etching solutions for examples and comparative examples
| Etching of the substrate | SEM drawing | Layering of cross sections | Taper angle | SEM drawing | |
| Example 1 | No corrosion | 1-1 | No delamination | 46.40° | 2-1 |
| Example 2 | No corrosion | - | No delamination | 53.8° | - |
| Example 3 | No corrosion | - | No delamination | 63.96° | - |
| Example 4 | No corrosion | - | No delamination | 71.75° | - |
| Example 5 | No corrosion | - | No delamination | 59.50° | - |
| Example 6 | No corrosion | - | Inner shrinking of aluminum layer | - | 2-2 |
| Comparative example 1 | No corrosion | - | Inner shrinking of aluminum layer | - | 2-3 |
| Comparative example 2 | Corrosion by corrosion | 1-2 | No delamination | 66.71° | 2-4 |
As can be seen from Table 2, the titanium-aluminum-titanium composite film layers in examples 1 to 5 can be etched effectively, and the taper angle of the etched film layer is good, and no delamination phenomenon occurs; in the embodiment 6, thiosulfate is used, but pyrosulfate is not used, so that the corrosion speed of the aluminum film is high, and the titanium film is corroded slowly, so that the aluminum film is shrunk inwards; comparative example 1 used pyrosulfate but not thiosulfate, which also caused aluminum film corrosion rate faster than titanium film and aluminum layer shrinkage; comparative example 2 the titanium film was effectively etched by the addition of fluoride, and the etched film layer was not delaminated, but the presence of fluoride caused corrosion of the substrate.
And (3) testing the stability of the etching solution: adding 6000ppm Ti powder and 6000ppm Al powder into the medicinal liquid, heating in 40deg.C water bath after dissolution, sampling to detect chromaticity of the medicinal liquid, recording temperature change of the medicinal liquid by a temperature recorder to confirm whether bumping, sampling to detect chromaticity of the medicinal liquid after 72 hr.
TABLE 3 stability of etching solutions
| Initial chroma value | Chromaticity value of 72hr | Whether or not to suddenly boil | Drawings | |
| Example 1 | 6.3 | 6.5 | Whether or not | 3-1 |
| Example 2 | 6.2 | 6.3 | Whether or not | - |
| Example 3 | 6.6 | 6.4 | Whether or not | - |
| Example 4 | 6.1 | 6.2 | Whether or not | - |
| Example 5 | 6.4 | 6.5 | Whether or not | - |
| Example 6 | 6.6 | 6.7 | Whether or not | - |
| Comparative example 1 | 6.4 | 6.5 | Whether or not | - |
| Comparative example 2 | 6.5 | 6.6 | Is that | 3-2 |
As is clear from Table 3, examples 1 to 6 and comparative examples 1 to 2 were heated at 40℃for 72 hours after adding Ti and Al powders, and the color of the medicinal liquid was not substantially changed; examples 1-6 and comparative examples 1-2 were heated at 40 ℃ for 72 hours after Ti and Al powders were added, the liquid medicine was free from bumping, and comparative example 2 was boiled for 2634 minutes with a sudden increase in the liquid medicine temperature, thus demonstrating that thiosulfate and pyrosulfate had the effect of increasing the stability of the etching solution and preventing the bumping of the etching solution.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (4)
1. An acidic etching solution for a titanium aluminum titanium composite film layer is characterized in that: including oxidizing acids, non-oxidizing acids, thiosulfates, pyrosulfates and deionized water;
the acid etching solution comprises, by mass, 100% of oxidizing acid, 15% to 30% of non-oxidizing acid, 0.2% to 2% of thiosulfate, 0.5% to 3% of pyrosulfate and the balance of deionized water;
the oxidizing acid is one or a combination of more of nitric acid, hydroiodic acid, perchloric acid, nitrous acid and chromic acid;
the non-oxidizing acid is one or a combination of more of hydrochloric acid, sulfuric acid and phosphoric acid.
2. The acidic etching solution for the titanium-aluminum-titanium composite film layer according to claim 1, wherein the acidic etching solution is characterized in that: the thiosulfate is one or two of sodium thiosulfate and potassium thiosulfate.
3. The acidic etching solution for the titanium-aluminum-titanium composite film layer according to claim 1, wherein the acidic etching solution is characterized in that: the pyrosulfate is one or two of sodium pyrosulfate and potassium pyrosulfate.
4. The method for preparing the acidic etching solution for the titanium-aluminum-titanium composite film layer according to claim 1, which is characterized in that: adding deionized water into the oxidizing acid, stirring uniformly, slowly adding the non-oxidizing acid in a stirring state, stirring uniformly again, adding thiosulfate and pyrosulfate, stirring to dissolve, and then filtering the mixed solution by suction, and collecting filtrate to obtain the acidic etching solution.
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| CN114381735A (en) * | 2022-01-19 | 2022-04-22 | 东莞奕创表面处理科技有限公司 | Preparation and application of aluminum etchant |
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| US7147798B2 (en) * | 2003-08-22 | 2006-12-12 | Arch Specialty Chemicals, Inc. | Aqueous based metal etchant |
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| DE102005020558A1 (en) * | 2004-05-19 | 2005-12-15 | Heidelberger Druckmaschinen Ag | Process to render print cylinder re-usable by surface softening with plasma followed by removal by abrasion and solvents |
| CN105297022A (en) * | 2014-07-24 | 2016-02-03 | 关东化学株式会社 | Etching liquid composition and etching method |
| CN104152903A (en) * | 2014-09-02 | 2014-11-19 | 冯书通 | A method of generating root nodule-shaped microholes in a metallic material surface |
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